CN112547314B - Full-quantity resource production method of siliceous and silicate refractory collophanite - Google Patents
Full-quantity resource production method of siliceous and silicate refractory collophanite Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
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- B03D1/08—Subsequent treatment of concentrated product
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/04—Waste materials; Refuse
- C04B18/14—Waste materials; Refuse from metallurgical processes
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- C04B18/145—Phosphorus slags
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Abstract
The invention discloses a full resource production method of siliceous and silicate refractory collophanite, and relates to the technical field of collophanite processing. Grinding collophanite, adding water glass and a collecting agent, and performing direct flotation; flotation foam is used as phosphate concentrate for preparing acid by wet-process phosphoric acid, underflow tailings are diluted by water and then separated, and sodium hydroxide solution is added into coarse fraction tailings to prepare liquid sodium silicate with the modulus of 2.2-2.4; one part is used for direct flotation, sulfuric acid is added into the residual liquid water glass to prepare white carbon black, and the white carbon black is used for wet phosphoric acid defluorination; and adding a polymeric flocculant into the fine-particle tailings to prepare the building brick. The method combines ore dressing and chemical industry to classify the positive flotation tailings, so that coarse fraction tailings are prepared into water glass serving as a positive flotation inhibitor, and the water glass is further processed to produce white carbon black serving as a defluorinating agent. The fine-grained tailings are used for producing building bricks, flotation tailings are not generated any more, and the full resource utilization of siliceous and silicate refractory collophanite is realized.
Description
Technical Field
The invention relates to the technical field of collophanite processing, in particular to a full-scale resource production method of siliceous and silicate refractory collophanite.
Background
Phosphate rock is an important component in agricultural fertilizers and phosphorus-based chemical preparations as a non-renewable resource. With the development of economy, the demand of phosphate ore is continuously and rapidly increasing. Although China is a large country of phosphorite resources, among the proved phosphorites, mainly sedimentary phosphorite (collophanite) accounts for 80% of the total amount, and most of the phosphorite is medium-low grade collophanite, and the ore has the characteristics of low grade, complex structure, fine disseminated particle size, difficult dissociation and the like. But the enrichment of phosphorus can be achieved by flotation. The phosphorus concentrate is floated and used for subsequent processing, the tailings are collected and then are piled in a tailing pond, a large amount of land and forest land needs to be acquired, and potential safety hazards of dam break exist. The tailings have complex components, so that a proper utilization way is difficult to find. However, in recent years, with the tightening of environmental protection policy, new tailings ponds are not allowed to be built, so that manufacturers have to search for a recycling method of tailings vigorously.
The siliceous and silicate refractory collophanite is P2O518-21 percent of content, less than 2 percent of MgO content and SiO2Content greater than 28% and Fe2O3Content of Al is more than 1.6%2O3Phosphate ore with content of more than 2.6% and SiO contained in the phosphate ore290% of the silica is present in the form of quartz and 10% in the form of silicate minerals. The collophanite flotation tailings are mainly siliceous minerals, specifically P2O5Less than 8% of SiO2Content of more than 60 percent and Fe2O3Content of more than 2 percent and Al2O3The content is more than 3 percent.
Patent CN107362910A discloses a method for preparing a phosphorite flotation regulator from direct flotation tailings, which uses the direct flotation tailings generated by siliceous phosphorite flotation and the product (mainly water glass) obtained by reaction with non-polar alkali as the phosphorite direct flotation desilication regulator. But the tailings also contain mud and other impurities, and the mud and other impurities are all used for manufacturing water glass and are easy to block a filtering system.
Disclosure of Invention
The invention aims to provide a full-quantity resource production method of siliceous and silicate refractory collophanite, which solves the problem that tailings after flotation are difficult to recycle.
In order to solve the technical problems, the invention adopts the following technical scheme: a full-quantity resource production method of siliceous and silicate refractory collophanite is characterized by comprising the following steps:
(1) grinding collophanite until the content of the collophanite is more than 80 percent and the fineness is-0.074 mm to obtain raw material pulp with the pulp concentration of 26-30 percent;
(2) adding water glass and a collecting agent into the raw ore pulp and then performing positive flotation operation;
(3) flotation foam is used as phosphate concentrate for preparing acid by wet-process phosphoric acid, and underflow tailings are diluted by water and then separated to obtain coarse fraction tailings and fine fraction tailings;
(4) modulating the coarse fraction tailings into 30-50% of ore pulp, pumping the ore pulp into a high-pressure reaction kettle, adding a sodium hydroxide solution, and reacting at the temperature of 130-170 ℃ for 3-4 hours to prepare liquid water glass with the modulus of 2.2-2.4;
(5) 50-70% of the liquid water glass in the step (4) is used in the step (2), sulfuric acid is added into the residual liquid water glass, acid leaching is carried out for 7-10 hours at the temperature of 70-80 ℃, and white carbon black is prepared after neutralization, filtration, washing and drying and is used for defluorination of wet-process phosphoric acid in the step (3);
(6) adding a polymeric flocculant into the fine-particle tailings, settling, concentrating and drying to prepare a building brick, settling, concentrating and drying until the water content is less than 5%, stirring with cement, and conveying to a brick making machine at 800-1000 t/m2Pressing and forming under pressure, and airing to obtain the building brick.
According to a further technical scheme, the addition amount of the water glass is 3-10 kg/t of raw ore, the collecting agent is YP6-3, and the addition amount is 1-3 kg/t of raw ore.
The further technical scheme is that the underflow tailings in the step (3) are diluted to the concentration of 10% -20% by adding water, and a high-speed centrifuge is used for separating for 5-10 min at the rotating speed of 1000-1400 r/min.
According to a further technical scheme, in the step (4), the concentration of the sodium hydroxide solution is 25% -30%, and the mass ratio of the ore pulp to the sodium hydroxide solution is 1: 1.33-1.5.
According to a further technical scheme, in the step (5), the concentration of sulfuric acid is 30% -35%, and the mass ratio of liquid water glass to sulfuric acid is 1: 0.8-1.
In a further technical scheme, the molecular weight of the high molecular flocculant in the step (6) is 1400-2000 ten thousand, and the addition amount is 30-50 g/t.
The reaction mechanism is as follows: separating the positive flotation tailings into coarse and fine size fractions through centrifugation. Since quartz is difficult to grind, coarse fraction tailings (P) are mainly present2O5The content is less than 8 percent, SiO2Content greater than 80%, Fe2O3Less than 1% of Al2O3Content less than 1%), while clay mineral has low hardness, is easy to grind, and is mainly distributed in fine fraction (P)2O5Less than 8% of SiO2Less than 60% of Fe2O3More than 2.5% of Al2O3Content greater than 4%). After centrifugal separation, the concentration of coarse fraction reaches the process requirement of producing water glass, while the concentration of fine fraction is low and needs flocculating agent to concentrate to improve the concentration, so as to reduce the production cost of subsequent drying raw material brick making.
Compared with the prior art, the invention has the beneficial effects that: through the combination of ore dressing and chemical industry, after the positive flotation tailings are classified, the water glass prepared by producing coarse-grained siliceous gangue (mainly quartz) in the tailings is recycled as a positive flotation inhibitor, and the water glass is further processed to produce white carbon black as an additive for removing harmful impurities in the production process of phosphorus chemical industry. The fine-grained gangue minerals are used for producing the building bricks, flotation tailings are not generated, full resource utilization of siliceous and silicate refractory collophanite is realized, waste of tailing resource stockpiling is avoided, and meanwhile, the building bricks prepared from the redundant water glass and white carbon black can be used as products to bring certain economic benefits.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
(1) For P in siliceous and silicate refractory collophanite2O519.5% of MgO, 0.8% of SiO2The content of Fe is 38% (90% in quartz form and 10% in silicate mineral form)2O3Content of 1.6% and Al2O3The content is 2.6 percent, the ore is ground until the content of the ore with the fineness of-0.074 mm is 80 percent, and raw material ore pulp with the ore pulp concentration of 26 percent to 30 percent is obtained. Adding water glass into raw ore of 3-8 kg/t, adding a collecting agent YP6-3 into the raw ore of 1-2 kg/t, and carrying out direct flotation operation on the collophanite through pulp mixing and mineralization.
(2) Flotation froth is P2O530% of MgO, 0.9% of SiO2The phosphate concentrate with the content of 18 percent is used for preparing acid by wet-process phosphoric acid after concentration to produce a fertilizer product or a calcium feed product.
(3) P in positive flotation tailings (the fineness is 0.038mm, and the content accounts for 90 percent)2O56.5% of SiO2The content of the raw materials is 75 percent, the raw materials are diluted by adding water until the concentration of ore pulp is 10 percent, the raw materials enter a high-speed centrifuge (the rotating speed is 1200r/min) to separate the ore mud and the quartz for 5 to 8min, and a coarse fraction material product (P) accounting for 80 percent is obtained2O58% of SiO292% of Fe2O30.5% of Al2O3Content of 0.6%) and 20% of fine fraction material product (P)2O54.5% of SiO220% of Fe2O3Content 3.5% Al2O3Content 8%).
(4) Controlling the concentration of a coarse fraction product at 50%, pumping the coarse fraction product into a high-pressure reaction kettle, adding a 30% sodium hydroxide solution according to the mass ratio of 1:1.45, introducing steam for reaction under the condition of stirring, controlling the temperature at 160 ℃, and generating liquid water glass with the modulus of 2.4.
(5) Returning 60% liquid water glass to the direct flotation operation to be used as a direct flotation inhibitor, and mixing the remaining 40% liquid water glass with a 30% sulfuric acid solution according to the weight ratio of 1: 2.4 (mass ratio), acid leaching for 10 hours at the temperature of about 80 ℃, neutralizing, filtering, washing and drying to obtain the white carbon black with the purity of 93 percent.
(6) Adding a polymeric flocculant into the fine-particle tailings, settling, concentrating and drying until the water content is less than 5%, stirring with cement, and then conveying into a brick making machine at a speed of 800-1000 t/m2Pressing and forming under pressure, and airing to obtain the building brick, wherein the molecular weight of the polymeric flocculant is 1400-2000 ten thousand, and the addition amount is 30-50 g/t.
Example 2
(1) For P in siliceous and silicate refractory collophanite2O520% of MgO, 1.5% of SiO2The content of Fe is 35% (90% in quartz form and 10% in silicate mineral form)2O3Content of 1.7% and Al2O3The content is 2.8 percent, the ore is ground until the content of the ore with the fineness of-0.074 mm is 98 percent, and raw material ore pulp with the ore pulp concentration of 26 percent to 30 percent is obtained. Adding water glass into raw ore of 3-10 kg/t, adding a collecting agent YP6-3 into the raw ore of 1-3 kg/t, and carrying out direct flotation operation on the collophanite through pulp mixing and mineralization.
(2) Flotation froth is P2O530.5% of MgO, 0.5% of SiO2The phosphate concentrate with the content of 20 percent is used for preparing acid by wet-process phosphoric acid after concentration to produce a fertilizer product or a calcium feed product.
(3) P in positive flotation tailings (the fineness is 0.038mm, and the content accounts for 90 percent)2O57% of SiO2The content of 68 percent, water is added to dilute the mixture until the concentration of the ore pulp is 15 percent, the mixture enters a high-speed centrifuge (the rotating speed is 1300r/min) to separate the ore mud and the quartz, and a coarse fraction material product (P) accounting for 75 percent is obtained2O5Content 9% SiO288% of Fe2O30.5% of Al2O3Content 0.8%) and 25% of the product (P) of the fine fraction2O55% of SiO225% of Fe2O33% of Al2O3Content (wt.)7％)。
(4) Controlling the concentration of a coarse fraction product at 40%, pumping the coarse fraction product into a high-pressure reaction kettle, adding a 30% sodium hydroxide solution according to the mass ratio of 1:1.38, introducing steam for reaction under the condition of stirring, controlling the temperature at 160 ℃, and generating liquid water glass with the modulus of 2.3.
(5) Returning 50% of liquid water glass to the positive flotation to be used as a positive flotation inhibitor, and mixing the residual liquid water glass with 33% sulfuric acid according to the weight ratio of 1: 2.3 (mass ratio), acid leaching for 9 hours at about 80 ℃, neutralizing, filtering, washing and drying to obtain the white carbon black with the purity of 92 percent.
(6) And adding a polymeric flocculant into the fine-particle tailings, settling, concentrating and drying to prepare the building brick, wherein the molecular weight of the polymeric flocculant is 1400-2000 ten thousand, and the addition amount is 30-50 g/t.
Example 3
(1) For P in siliceous and silicate refractory collophanite2O518% of MgO, 2% of SiO2The content of 28% (90% in quartz form, 10% in silicate mineral form), Fe2O3Content of 1.6% and Al2O3The content is 2.8 percent, the ore is ground until the content of the ore with the fineness of-0.074 mm is 98 percent, and raw material ore pulp with the ore pulp concentration of 26 percent to 30 percent is obtained. Adding water glass according to 3-10 kg/t of raw ore, adding a collecting agent YP6-3 according to 1-3 kg/t of raw ore, and carrying out pulp mixing mineralization to carry out collophanite direct flotation operation.
(2) Flotation froth is P2O528.5% of MgO, 0.8% of SiO2The phosphate concentrate with the content of 18 percent is used for preparing acid by wet-process phosphoric acid after concentration to produce a fertilizer product or a calcium feed product.
(3) P in positive flotation tailings (the fineness is 0.038mm, and the content accounts for 90 percent)2O55.5% of SiO2The content of the coarse fraction is 63 percent, the coarse fraction is diluted by adding water until the concentration of the ore pulp is 20 percent, and the ore pulp enters a high-speed centrifuge (the rotating speed is 1400r/min) for separating ore mud and quartz, so that a coarse fraction material product (P) accounting for 70 percent is obtained2O5Content 6% SiO285% of Fe2O30.5% of Al2O3Content 0.8%) and 30% of fine fraction material product (P)2O56.3% of SiO2Content 24% of Fe2O33% of Al2O3Content 6%).
(4) Controlling the concentration of a coarse fraction product to be 45%, pumping the coarse fraction product into a high-pressure reaction kettle, adding 30% liquid alkali in a material ratio of 1:1.33 (mass ratio), introducing steam for reaction under the condition of stirring, controlling the temperature to be 160 ℃, and generating liquid water glass with the modulus of 2.2.
(5) Returning a part of liquid water glass to the positive flotation to be used as a positive flotation inhibitor, and mixing a part of liquid water glass with 35% sulfuric acid according to the weight ratio of 1: 2.3 (mass ratio), acid leaching for 8 hours at about 80 ℃, neutralizing, filtering, washing and drying to obtain the white carbon black with the purity of 90 percent.
(6) And adding a polymeric flocculant into the fine-particle tailings, settling, concentrating and drying to prepare the building brick, wherein the molecular weight of the polymeric flocculant is 1400-2000 ten thousand, and the addition amount is 30-50 g/t.
Although the invention has been described herein with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure. More specifically, various variations and modifications are possible in the component parts or arrangements of the subject combination arrangement within the scope of the disclosure, the drawings and the appended claims. In addition to variations and modifications in the component parts or arrangements, other uses will also be apparent to those skilled in the art.
Claims (6)
1. A full-quantity resource production method of siliceous and silicate refractory collophanite is characterized by comprising the following steps:
(1) grinding collophanite until the content of the collophanite is more than 80 percent and the fineness is-0.074 mm to obtain raw material pulp with the pulp concentration of 26-30 percent;
(2) adding water glass and a collecting agent into the raw ore pulp and then performing positive flotation operation;
(3) flotation foam is used as phosphate concentrate for preparing acid by wet-process phosphoric acid, and underflow tailings are diluted by water and then separated to obtain coarse fraction tailings and fine fraction tailings;
(4) modulating the coarse fraction tailings into 30-50% of ore pulp, pumping the ore pulp into a high-pressure reaction kettle, adding a sodium hydroxide solution, and reacting at the temperature of 130-170 ℃ for 3-4 hours to prepare liquid water glass with the modulus of 2.2-2.4;
(5) 50-70% of the liquid water glass in the step (4) is used in the step (2), sulfuric acid is added into the residual liquid water glass, acid leaching is carried out for 7-10 hours at the temperature of 70-80 ℃, and white carbon black is prepared after neutralization, filtration, washing and drying and is used for defluorination of wet-process phosphoric acid in the step (3);
(6) adding a polymeric flocculant into the fine-particle tailings, settling, concentrating and drying until the water content is less than 5%, stirring with cement, and then conveying into a brick making machine at a speed of 800-1000 t/m2Pressing and forming under pressure, and airing to obtain the building brick.
2. The full-scale resource production method of siliceous and silicate refractory collophanite according to claim 1, characterized in that: the addition amount of the water glass is 3-10 kg/t of raw ore, the collecting agent is YP6-3, and the addition amount is 1-3 kg/t of raw ore.
3. The full-scale resource production method of siliceous and silicate refractory collophanite according to claim 1, characterized in that: and (4) adding water into the underflow tailings in the step (3) to dilute the underflow tailings to a concentration of 10% -20%, and separating for 5-10 min at a rotating speed of 1000-1400 r/min by using a high-speed centrifuge.
4. The full-scale resource production method of siliceous and silicate refractory collophanite according to claim 1, characterized in that: in the step (4), the concentration of the sodium hydroxide solution is 25-30%, and the mass ratio of the ore pulp to the sodium hydroxide solution is 1: 1.33-1.5.
5. The full-scale resource production method of siliceous and silicate refractory collophanite according to claim 1, characterized in that: the concentration of sulfuric acid in the step (5) is 30-35%, and the mass ratio of the liquid water glass to the sulfuric acid is 1: 0.8-1.
6. The full-scale resource production method of siliceous and silicate refractory collophanite according to claim 1, characterized in that: the molecular weight of the high molecular flocculant in the step (6) is 1400-2000 ten thousand, and the addition amount is 30-50 g/t.
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| JPS5717416A (en) * | 1980-07-04 | 1982-01-29 | Kyoei Kasei Kogyo Kk | Recovering method for silica from tailing of fluorite |
| SU1310377A1 (en) * | 1985-01-16 | 1987-05-15 | Ленинградский Технологический Институт Им.Ленсовета | Method for producing long-acting fertilizer |
| DE19835498A1 (en) * | 1998-08-06 | 2000-02-10 | Uvr Fia Gmbh Verfahrensentwick | Production of intensively colored lapis lazuli for direct use as pigment involves multistage flotation, using long-chain amine as collector and neutral to alkaline conditions for removing mica and recovering and purifying lapis lazuli |
| CN101713234B (en) * | 2009-10-30 | 2011-08-31 | 武汉理工大学 | Non-autoclaved and unburned brick and preparation method thereof |
| CN102424394B (en) * | 2011-09-11 | 2013-06-19 | 北京科技大学 | Process for preparing water glass from silicon micropowder by using wet method |
| CN102698873A (en) * | 2011-11-28 | 2012-10-03 | 云南磷化集团有限公司 | Beneficiation method for desorbing silicate impurities in collophanite through direct flotation |
| CN103657840A (en) * | 2013-07-10 | 2014-03-26 | 中蓝连海设计研究院 | Dry type discharge method of phosphorus ore tailings |
| CN103626471B (en) * | 2013-11-26 | 2015-12-02 | 武汉工程大学 | A kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce and preparation method thereof |
| CN103950911B (en) * | 2014-05-06 | 2016-03-16 | 云南磷化集团有限公司 | Slag acid and yellow phosphorus furnace slag is utilized to prepare the method for calcium hydrophosphate fodder coproduction water glass |
| CN105032601A (en) * | 2015-06-29 | 2015-11-11 | 江西省莲花山矿产实业有限公司 | Tailing disposal method |
| CN107362910A (en) * | 2017-08-30 | 2017-11-21 | 云南磷化集团有限公司 | A kind of method that direct flotation phosphorus mine tailing prepares phosphate rock floating regulator |
| CN111422878B (en) * | 2020-04-20 | 2023-03-07 | 武汉工程大学 | Method for treating silico-calcium collophanite |
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